将不同铝含量的聚铝硅氮烷前驱体在氮气保护下1200℃裂解,再在1400-1800℃高温处理,制备出非晶Si-Al-C-N.采用红外光谱、X射线衍射,拉曼光谱和透射电子显微镜分别表征前驱体的结构、Si-Al-C-N的析晶特性、自由碳的微观结构,研究了铝含量、析晶温度和保温时间对非晶Si-Al-C-N析晶性能的影响.结果表明:具有不同铝含量的非晶Si-Al-C-N在1400℃处理后仍为非晶状态,但发生组份偏析形成自由碳；在1500℃出现纳米级β-Si3N4和α-Si3N4晶体；在1600℃α-Si3N4转变为β-Si3N4,并析出微量α-SiC和2H-SiC/AlN固溶体型晶核；在1700℃除β-Si3N4外,还析出大量2H-SiC/AlN固溶体和部分α/β-SiC晶体,铝含量最低的Si-Al-C-N陶瓷中的β-Si3N4消失；在1800℃,只含有β-SiC和2H-SiC/AlN固溶体晶体,但是发生了相分离并分别形成富AlN和富SiC固溶体区.铝含量的增加有利于晶体析出和晶体数量的增加.非晶SiAlCN在1500℃开始析出纳米晶,在1800℃处理后析出的晶体仍为纳米晶.高共价键非晶SiAlCN的高温析晶过程,是一个主要由热力学控制的过程.
参考文献
| [1] | P.Greil,M.Seibold,Modelling of dimensional changes during polymer-ceramic conversion for bulk component fabrication,Journal of Materials Science,27(9),1053(1992) |
| [2] | Peter Greil,Near net shape manufacturing of polymer derived ceramics,Journal of the European Ceramic Society,18(13),1905(1998) |
| [3] | G.Ziegler, H.J.kleebe, G.Motz, H.Miiller, S.TraBl,W.Weibelzahl,Synthesis,microstructure and properties of SiCN ceramics prepared from tailored polymers,Materials Chemistry and Physics,61(1),55(1999) |
| [4] | S.R.Shah,R.Raj,Mechanical properties of a fully dense polymer derived ceramic made by a novel pressure casting process,Acta Materialia,50(16),4093(2002) |
| [5] | S.Sarkar,A.Chunder,W.Fei,L.An,L.Zhai,Superhydrophobic mats of polymer-derived ceramic fibers,Journal of the American Ceramic Society,91(8),2751(2008) |
| [6] | L.An,Y.Wang,L.Bharadwaj,L.Zhang,Y.Fan,D.Jiang,Y.Sohn,V.H.Desai,J.Kapat,L.C.Chow,Silicoaluminum carbonitride with anomalously high resistance to oxidation and hot corrosion,Advanced Engineering Materials,5(6),337(2004) |
| [7] | Y.Wang,L.An,Oxidation of polymer-derived SiAlCN ceramics,Journal of the American Ceramic Society,88(11),3075(2005) |
| [8] | Y.Wang,W.Fei,L.An,Oxidation/corrosion of polymerderived SiA1CN ceramics in water vapor,Journal of the American Ceramic Society,89(3),1079(2006) |
| [9] | Y.Wang,Y.Fan,L.Zhang,W.Zhang,L.An,Polymerderived SiA1CN ceramics resist oxidation at 1400 ℃,Scripta Materialia,55(4),295(2006) |
| [10] | K.J.L.Paciorek,J.H.Nakahara,L.A.Hoferkamp,C.George,J.L.Flippen-Anderson,R.Gilardi,W.R.Schmidt,Reaction of tris[bis(trimethylsilyl)amino]aluminum with ammonia and pyrolysis studies,Chemistry of Materials,3(1),82(1991) |
| [11] | G.Verdecia, K.L.O'Brien, W.R.Schmidt, T.M.Apple,Aluminum-27 and silicon-29 solid-state nuclear magnetic resonance study of silicon carbide/aluminum nitride systems:effect of silicon/aluminum ratio and pyrolysis temperature,Chemistry of Materials,10(4),1003(1998) |
| [12] | H.Nakashima,S.Koyama,K.Kuroda,Y.Sugahara,Conversion of a precursor derived from cage-type and cyclic molecular building blocks into Al-Si-N-C ceramic composites,Journal of the American Ceramic Society,85(1),59(2002) |
| [13] | R.Toyoda,S.Kitaoka,Y.Sugahara,Modification of perhydropolysilazane with aluminum hydride:preparation of poly(aluminasilazane)s and their conversion into Si-Al-N-C ceramics,Journal of the American Ceramic Society,28(1),271(2008) |
| [14] | F.Berger,M.Weinmann,F.Aldinger,K.Müller,Solid-state NMR studies of the preparation of Si-Al-C-N ceramics from aluminum-modified polysilazanes and polysilylcarbodiimides,Chemistry of Materials,16(5),919(2004) |
| [15] | YANG Nanru,Test Methods of Inorganic Non-metallic Materials (Wuhan, Wuhan University of Technology Press,2003) p.91(杨南如,无机非金属材料测试方法(武汉,武汉理工大学出版社,2003)p.91) |
| [16] | Y.Mori,Y.Sugahara, Pyrolytic conversion of an Al-Si-N-C precursor prepared via hydrosilylation between[Me(H)SiNH]4 and[HAlN(allyl)]m[HAlN(ethyl)]n,Applied Organometallic Chemistry,20(8),527(2006) |
| [17] | A.Müller, P.Gerstel, E.Butchereit, K.G.Nickel,F.Aldinger, Si/B/C/N/Al precursor-derived ceramics:synthesis,high temperature behaviour and oxidation resistance,Journal of the European Ceramic Society,24(12),3409(2004) |
| [18] | W.R.Schmidt, D.M.Narsavage-Heald, D.M.Jones,P.S.Marchetti,D.Raker,G.E.Maciel,Poly(borosilazane)precursors to ceramics nanocomposites,Chemistry of Materials,11(6),1455(1999) |
| [19] | J.Lücke,J.Hacker,D.Suttor,G.Ziegler,Synthesis and characterization of silazane-based polymers as precursors for ceramic matrix composites,Applied Organometallic Chemistry,11(2),181(1997) |
| [20] | W.Rafaniello,K.Cho,A.V.Virkar,Fabrication and characterization of SiC-AlN alloys,Journal of Materials Science,16(12),3479(1981) |
| [21] | M.Miura,T.Yogo,S.Hirano,Phase separation and toughening of SiC-AlN solid-solution ceramics,Journal of Materials Science,28(14),3859(1993) |
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